title: Development and validation of a RP-HPLC method for stability-indicating assay of gemifloxacin mesylate including identification of related substances by LC-ESI-MS/MS, 1H and 13C NMR spectroscopy.
abstract: A validated stability indicating RP-HPLC assay of gemifloxacin mesylate was developed by separating its related substances on an Inertsil-ODS3V-C18 (4.6 × 250 mm; 5 μm) column using 0.1% trifluoroaceticacid (pH 2.5) and methanol as a mobile phase in a gradient elution mode at a flow rate of 1.0 mL/min at 27°C. The column effluents were monitored by a photodiode array detector set at 287 nm. The method was validated in terms of accuracy, precision and linearity as per ICH guidelines. Forced degradation of gemifloxacin (GFX) was carried out under acidic, basic, thermal, photolysis and peroxide conditions and the degradation products were separated and characterized by ESI-MS/MS, (1) H and (13) C NMR spectroscopy. The method was successfully applied to the analysis of bulk drugs and the recoveries of gemifloxacin and impurities were in the range of 97.60-102.90 and 96.99-102.10%, respectively. No previous reports were found in the literature on identification of degradation products of gemifloxacin.
authors.affiliation: Analytical Chemistry Division, Discovery Laboratory, Indian Institute of Chemical Technology, Tarnaka, Hyderabad, 500 607, India. rnrao55@yahoo.com, rnrao@iict.res.in.
authors.forename: R Nageswara
authors.initials: RN
authors.lastname: Rao
authors.forename: Ch Gangu
authors.initials: ChG
authors.lastname: Naidu
authors.forename: K Guru
authors.initials: KG
authors.lastname: Prasad
authors.forename: R
authors.initials: R
authors.lastname: Narasimha
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D056148:Chromatography, Reverse-Phase / Q000379:methods; D004340:Drug Contamination; D024841:Fluoroquinolones / Q000032:analysis* / Q000737:chemistry*; D000077735:Gemifloxacin; D016014:Linear Models; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D009287:Naphthyridines / Q000032:analysis* / Q000737:chemistry*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D024841:Fluoroquinolones; D009287:Naphthyridines; D000077735:Gemifloxacin